HCID 69733344, Verbindung → HCID 10067963, Verbindung

HRID 966104Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 966104
Cl.[OH:2][C:3]1[C:4]([O:27][CH3:28])=[C:5]([C:10](=[O:26])[CH2:11][NH:12][C:13]([CH3:25])([CH3:24])[CH2:14][C:15]2[C:20]([CH3:21])=[CH:19][C:18]([CH3:22])=[CH:17][C:16]=2[CH3:23])[CH:6]=[CH:7][C:8]=1[OH:9]>CO.[Pt](=O)=O>[CH3:25][C:13]([NH:12][CH2:11][CH:10]([C:5]1[C:4]([O:27][CH3:28])=[C:3]([OH:2])[C:8]([OH:9])=[CH:7][CH:6]=1)[OH:26])([CH3:24])[CH2:14][C:15]1[C:20]([CH3:21])=[CH:19][C:18]([CH3:22])=[CH:17][C:16]=1[CH3:23]

Komponenten

4

Edukt 1

HCID 69733344HCID 69733344, Verbindung

Produkt 1

HCID 10067963HCID 10067963, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 345198Adams' catalystKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

9 g of 1-(3,4-dihydroxy-2-methoxyphenyl)-2-[1,1-dimethyl-2-(2,4,6-trimethylphenyl)-ethylamino]ethanone hydrochloride is hydrogenated with 0.4 g of platinum(IV) oxide in 125 mL of methanol. The catalyst is filtered off and the solvent is distilled off under reduced pressure. The residue is dissolved in 50 mL of ethyl acetate and the precipitated crystals are suction filtered and washed with diethyl ether and ethyl acetate. Yield: 6 g (67%, hydrochloride); melting point: 98° C.-105° C.

Aufarbeitung

  1. filtrationThe catalyst is filtered off
  2. distillationthe solvent is distilled off under reduced pressure
  3. dissolutionThe residue is dissolved in 50 mL of ethyl acetate
  4. filtrationfiltered
  5. washwashed with diethyl ether and ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-74c2ff880a7240749afd9141298e556e
Quelldatensatz
uspto-grants-2005_10
Patentnummer
US06951888B2

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